Flame-retardant anti-dripping copolymer nylon as well as preparation method and application thereof

A technology of copolymerized nylon and anti-melting drop, applied in the field of copolymerized nylon and its preparation and application, can solve the problems of inability to solve the problem of nylon melting, deteriorate the spinnability of materials, and burn the flame-retardant nylon, and achieve excellent flame retardant and anti-corrosion properties. Melting drop, inhibition of organic small molecule volatilization, high flame retardant efficiency

Pending Publication Date: 2022-01-11
SICHUAN UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Although the method of physical blending can effectively improve the flame retardancy of the obtained material (Ind.Eng.Chem.Res., 2013,52,2875-2886; 1697.), but the addition of a large amount of flame retardants will seriously deteriorate the spinnability of the material, limiting its use as a fiber, and can only be used as an engineering plastic
The chemical copolymerization method usually introduces phosphorus-containing groups into the nylon molecular chain to achieve flame retardancy, but phosphorus-containing copolymerized nylon usually achieves flame retardancy through the mechanism of promoting melting droplets (Polym. Adv. Technol., 2018, 29, 951-960 ; RSC Adv., 2018, 8, 9261-9271; Modern Textile Technology, 2016, 6, 13-18), it can not solve the problem of nylon droplet, thus making the obtained flame retardant nylon still easy to cause personal injury in a fire Burns, not less dangerous

Method used

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  • Flame-retardant anti-dripping copolymer nylon as well as preparation method and application thereof
  • Flame-retardant anti-dripping copolymer nylon as well as preparation method and application thereof
  • Flame-retardant anti-dripping copolymer nylon as well as preparation method and application thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0055] 146g (1mol) of adipic acid and 116g (1mol) of hexamethylenediamine were dissolved in ethanol, reacted at 90°C to form a salt and precipitated, and were filtered and dried to form a 50wt% aqueous solution; 14.2g (0.05mol) of 5 -(3-Hydroxystyryl)isophthalic acid and 5.8g (0.05mol) of hexamethylenediamine were dissolved in ethanol, reacted at 90°C to form a salt, and then precipitated, filtered and dried to form a 50wt% aqueous solution. Add the two aqueous solutions into the reactor, raise the temperature to 230°C, pressurize to 2.2MPa, and carry out the prepolymerization reaction under these conditions for 1.5h. Subsequently, the water vapor in the system was gradually discharged, and when the pressure in the system dropped to normal pressure, the vacuum was started to 4000 Pa and the temperature of the system was gradually raised, and the polycondensation reaction was carried out at 260° C. for 1 hour to obtain the product.

[0056] The intrinsic viscosity [η] of the co...

Embodiment 2

[0058] 105.6g (1.2mol) butanediamine, 96g (2.4mol) sodium hydroxide and 5g tetrabutylammonium chloride were dissolved in 1L of secondary water to configure solution A; 183g (1mol) adipoyl chloride and 60.6g ( 0.2mol) of 5-phenylethynyl isophthaloyl chloride was dissolved in 2L of dichloromethane to prepare solution B. Weigh solution A and solution B so that the number of moles of all diamines: the number of moles of all dibasic acid chlorides = 1:1; under rapid stirring at 2000rpm, quickly pour solution B into solution A, and continue stirring for 30 minutes to complete A large number of fibrous solids were precipitated during polymerization, and the product was obtained after suction filtration, washing and drying.

[0059] The intrinsic viscosity [η] of the copolymerized nylon is 1.21dL / g; the oxygen index is 34.2%, the vertical combustion grade V-0 does not melt, the tensile strength is 62MPa, and the tensile modulus is 1884MPa.

Embodiment 3

[0061] 146g (1mol) of adipic acid and 102g (1mol) of pentamethylenediamine were dissolved in ethanol, reacted at 90°C to form a salt and precipitated out, and were filtered and dried to form a 70wt% aqueous solution; 21.1g (0.1mol) of 4 '-Aminobenzylidene-4-aminoaniline and 16.6g (0.1mol) of adipic acid were dissolved in ethanol, reacted at 90°C to form a salt, and then precipitated. After filtering and drying, it was configured into a 70wt% aqueous solution. First add the two aqueous solutions into the reaction kettle, then add adipic acid, and make the moles of all diamines: the moles of all dibasic acids = 0.8:1, raise the temperature to 220°C, pressurize to 1.6MPa, Under these conditions, the prepolymerization reaction was carried out for 2h. Subsequently, the water vapor in the system was gradually discharged, and when the pressure in the system dropped to normal pressure, vacuuming was started to 5000 Pa and the temperature of the system was gradually raised, and the pol...

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Abstract

Flame-retardant anti-dripping copolymer nylon disclosed by the invention is composed of structural units represented by I, II, IV or III and IV, wherein the number of the structural units of IV is 1-99% of the number of the structural units of I, and the ratio of the number of the structural units of II to the number of the structural units of I and IV is 1; or the number of the structural units of IV is 1-99% of the number of the structural units of II, and the ratio of the number of the structural units of I to the number of the structural units of II and IV is 1; or the number of structural units of IV is 1-99% of the number of structural units of III. The intrinsic viscosity [eta] of the copolymer nylon is 0.52-1.35 dL/g, and the limit oxygen index of the copolymer nylon is 25.3-36.4%; the vertical combustion grade is V-2 to V-0; the tensile strength is 47-84 MPa; and the tensile modulus is 1487-2294 MPa. The invention also discloses a preparation method of the copolymer nylon. The flame-retardant monomer is very stable at processing and synthesis temperatures and does not interact or be decomposed, so that the thermoplastic processability of the obtained nylon is retained, chemical interaction can be generated at a higher temperature or during combustion, melt dripping can be inhibited, charring of the melt can be promoted, and the copolymer nylon is endowed with excellent flame-retardant and anti-molten-drop effects. The process is mature and easy to control and industrialize.

Description

technical field [0001] The invention belongs to the technical field of copolymerized nylon and its preparation and application. In particular, it relates to a class of copolymerized nylon (including petroleum-based nylon and bio-based nylon) with flame retardancy and droplet resistance, and a preparation method and application thereof. This type of copolymerized nylon can obtain better flame retardant and droplet resistance properties through the special chemical reaction of flame retardant monomers at high temperatures. Background technique [0002] Nylon (also known as polyamide, abbreviated as PA) is a thermoplastic material with excellent performance. It has excellent mechanical properties, chemical corrosion resistance, abrasion resistance, etc. It is widely used as engineering plastics and fibers, and is used in daily life. and all areas of the national economy. In recent years, in addition to the traditional petroleum-based nylon, bio-based nylon has also received m...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08G69/26C08G69/28C08G69/36C08L77/06C08L77/00C08J5/18
CPCC08G69/265C08G69/28C08G69/36C08L77/06C08L77/00C08J5/18C08J2377/06C08J2377/00C08L2203/16C08L2203/12C08L2201/02C08L2201/08
Inventor 王玉忠刘博文张琴何凤鸣陈力郭德明
Owner SICHUAN UNIV
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